CN103035924B - Anode slurry of high-rate lithium ion battery and fabrication method of anode slurry - Google Patents
Anode slurry of high-rate lithium ion battery and fabrication method of anode slurry Download PDFInfo
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- CN103035924B CN103035924B CN201210591170.2A CN201210591170A CN103035924B CN 103035924 B CN103035924 B CN 103035924B CN 201210591170 A CN201210591170 A CN 201210591170A CN 103035924 B CN103035924 B CN 103035924B
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Abstract
The invention discloses anode slurry of a high-rate lithium ion battery and a fabrication method of the anode slurry. The fabrication method comprises the steps of mixing a binder, a conductive agent and a lithium iron phosphate active substance uniformly at a mass ratio of 1:(0.8-1.2):(18-23) with a mixer at a rotating speed of 19-21r/min for 2-4h, adding the uniformly mixed raw materials into an air blowing oven for baking at 80-90 DEG C for 8-12h, turning off the air blowing oven, cooling the mixed raw materials naturally to below 45 DEG C for use, adding the raw materials into a stirring barrel containg NMP (N-Methyl Pyrrolidone) in three times, stirring with a planetary stirrer, controlling the solid content of the slurry to be 30%-40%, stirring for 5-10min at a low speed and 1-1.5h at a high speed when the mixed raw materials are added in the first time and the second time, stirring for 5-10min at the low speed and 2-3h at the high speed when the mixed raw materials are added in the third time, adding NMP to adjust viscosity, controlling the viscosity to be 5000-10000MPa*s, stirring at the low speed to conduct vacuum defoaming, and filtering the slurry with a screen with 200 meshes.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to a kind of anode slurry of high-rate and preparation method thereof.
Background technology
The advantage such as ferric phosphate lithium ion battery is high with its power density, have extended cycle life, security performance is good and environmentally friendly, makes it be with a wide range of applications in power technology field.Along with electric tool, minitype motivation equipment improve constantly each performance requirement of lithium ion battery, the properties of ferric phosphate lithium ion battery constantly gets a promotion.High multiplying power lithium ion battery raw material require to have good conductivity, people use the moderate electrically conductive graphite of specific area and conductive black as anode conductive agent usually to improve the multiplying power energy of battery, for the special good conductive agent of electric conductivity, then specific area is large especially, slurry properties for follow under tradition pulping process is poor, so the common conductive agent that traditional pulping process can only use specific area moderate.Tradition making beating mode is first by binding agent PVDF(Kynoar) join NMP(N-methyl pyrrolidone) be uniformly dispersed in solvent, then add conductive agent and stir, finally add lithium-iron phosphate active material and stir.The conductive agent specific area that electric conductivity is special good is large, not easily disperses, and does not improve the dispersiveness of material by reducing slurry solid content, slurry viscosity can be caused so on the low side, mixing speed is not easily too fast, and mixing speed greatly then shear stress is large, also can reduce the viscosity of slurry.So make the special good conductive agent of electric conductivity rationally be applied, finding can not affect slurry viscosity, makes slurry have excellent machinability and the short anode sizing agent preparation technology of mixing time is very important.
Summary of the invention
The object of this invention is to provide a kind of anode slurry of high-rate and preparation method thereof, the technical problem that solve finds rational anode sizing agent dispersion technology, improves processing characteristics and the high rate performance of lithium ion battery.
For achieving the above object, technical scheme of the present invention is:
A kind of anode slurry of high-rate, is characterized in that: by binding agent, conductive agent, lithium-iron phosphate active material 1:(0.8 ~ 1.2 in mass ratio): (18 ~ 23) mix with batch mixer, rotating speed 20 ± 1r/min, mixing time 2 ~ 4h.
According to described anode slurry of high-rate, it is characterized in that: the raw material mixed is put into air blast baking box 85 ± 5 DEG C baking 8 ~ 12h, close heating make mixed raw material naturally cool to less than 45 DEG C for subsequent use.
According to described anode slurry of high-rate, it is characterized in that: divided by raw material to join for three times in the agitator that NMP is housed and stir with planetary mixer, slurry solid content controls 30 ~ 40%; Add mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 1 ~ 1.5h for the first time, for the second time, third time adds mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 2 ~ 3h, and finally add NMP adjusting viscosity, viscosity controls at 5000 ~ 10000MPas; Stirring at low speed vacuum froth breaking, 200 mesh sieves crossed by slurry.
According to described anode slurry of high-rate, it is characterized in that: conductive agent is one or more in carbon nano-tube CNTs, Ketjen black ECP and superconductive carbon black 350G.
According to described anode slurry of high-rate, it is characterized in that: lithium-iron phosphate active material is rate lithium-iron phosphate active material.
A kind of anode slurry of high-rate preparation method, the steps include: binding agent PVDF, conductive agent, lithium-iron phosphate active material 1:(0.8 ~ 1.2 in mass ratio): (18 ~ 23) mix with V-type batch mixer, rotating speed 20 ± 1r/min, mixing time 2 ~ 4h, then mixed raw material is put into air blast baking box 85 ± 5 DEG C baking 8 ~ 12h, close heating make mixed raw material naturally cool to less than 45 DEG C for subsequent use, mixed raw material is divided in the agitator joining dress NMP for three times and stir with planetary mixer, first stirring at low speed after at every turn adding mixed raw material, start high-speed stirred after scraping wall and vacuumize, stirring at low speed revolution 20 ± 1r/min, rotation 1500 ± 50r/min, high-speed stirred revolution 25 ± 1r/min, rotation 2200 ± 50r/min, high-speed stirred vacuumizes and connects cool circulation water, suction-0.08 ~-0.09MPa, vacuum breaker degree 0 ~-0.01 MPa, slurry temperature controls slurry solid content below 50 DEG C and controls 30 ~ 40%, add mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 1 ~ 1.5h for the first time, for the second time, third time adds mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 2 ~ 3h, and finally add NMP adjusting viscosity, viscosity controls at 3000 ~ 6000MPas, stirring at low speed vacuum froth breaking, 200 mesh sieves crossed by slurry, obtain finely dispersed anode sizing agent.
Advantage of the present invention and effect are:
1. the present invention uses that particle diameter is little, specific area is large, the special good conductive agent of electric conductivity, and conductive agent plays the effect that liquid is protected in imbibition in the battery, and improves the high-rate discharge ability of battery.
2. the present invention first mixes raw material dry powder with batch mixer, and avoid separately by binding agent PVDF and NMP mix and blend, binding agent PVDF is suspended in nmp solvent and not easily disperses, the problem that mixing time is long.
3. the present invention first mixes raw material dry powder with batch mixer, and the conductive agent making specific area larger more easily mixes in nmp solvent with lithium-iron phosphate active material, shortens mixing time, reduces production cost.
4. the present invention first mixes raw material dry powder with batch mixer, and under guaranteeing the finely dispersed prerequisite of slurry, slurry viscosity can reach moderate, and slurry can have good processing characteristics.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Anode slurry of high-rate of the present invention, is characterized in that: by binding agent, conductive agent, lithium-iron phosphate active material 1:(0.8 ~ 1.2 in mass ratio): (18 ~ 23) mix with batch mixer, rotating speed 20 ± 1r/min, mixing time 2 ~ 4h; Described anode slurry of high-rate, is characterized in that: the raw material mixed is put into air blast baking box 85 ± 5 DEG C baking 8 ~ 12h, close heating make mixed raw material naturally cool to less than 45 DEG C for subsequent use; Described anode slurry of high-rate, is characterized in that: divided by raw material to join for three times in the agitator that NMP is housed and stir with planetary mixer, slurry solid content controls 30 ~ 40%; Add mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 1 ~ 1.5h for the first time, for the second time, third time adds mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 2 ~ 3h, and finally add NMP adjusting viscosity, viscosity controls at 5000 ~ 10000MPas; Stirring at low speed vacuum froth breaking, 200 mesh sieves crossed by slurry;
A kind of anode slurry of high-rate preparation method, the steps include: binding agent PVDF, conductive agent, lithium-iron phosphate active material 1:(0.8 ~ 1.2 in mass ratio): (18 ~ 23) mix with V-type batch mixer, rotating speed 20 ± 1r/min, mixing time 2 ~ 4h, then mixed raw material is put into air blast baking box 85 ± 5 DEG C baking 8 ~ 12h, close heating make mixed raw material naturally cool to less than 45 DEG C for subsequent use, mixed raw material is divided in the agitator joining dress NMP for three times and stir with planetary mixer, first stirring at low speed after at every turn adding mixed raw material, start high-speed stirred after scraping wall and vacuumize, stirring at low speed revolution 20 ± 1r/min, rotation 1500 ± 50r/min, high-speed stirred revolution 25 ± 1r/min, rotation 2200 ± 50r/min, high-speed stirred vacuumizes and connects cool circulation water, suction-0.08 ~-0.09MPa, vacuum breaker degree 0 ~-0.01 MPa, slurry temperature controls slurry solid content below 50 DEG C and controls 30 ~ 40%, add mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 1 ~ 1.5h for the first time, for the second time, third time adds mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 2 ~ 3h, and finally add NMP adjusting viscosity, viscosity controls at 3000 ~ 6000MPas, stirring at low speed vacuum froth breaking, 200 mesh sieves crossed by slurry, obtain finely dispersed anode sizing agent.
Binding agent PVDF in the present invention is the one in U.S. Solef5130, French Arkema761A, French Arkema HSV900.
Conductive agent in the present invention is one or more in carbon nano-tube CNTs, Ketjen black ECP, superconduction carbon black Ensaco 350G.
Embodiment 1
By 2.0kg binding agent PVDF(U.S. Solef PVDF5130), 3.0kg conductive agent carbon nano-tube (Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences carbon nano-tube TNCC), 45kg rate lithium-iron phosphate active material (Heter Electronics Group Co., Ltd. self-control LiFePO 4 material) V-type batch mixer VH-100(Nanjing Ke Dixin plant equipment Co., Ltd) mixing, rotating speed 10 ± 1r/min, mixing time 3h.Then mixed raw material is put into air blast baking box 85 ± 5 DEG C baking 10h, close heating make mixed raw material naturally cool to less than 45 DEG C for subsequent use, 92.8kgNMP is joined in 200L double-planet power mixer (Guangzhou good luck mixing apparatus Co., Ltd) agitator, then mixed raw material is divided to join for three times in double-planet power mixer agitator and stir, add the mixed raw material of about 1/3 at every turn, scrape wall after adding mixed raw material after first stirring at low speed 5min restart high-speed stirred and vacuumize at every turn, stirring at low speed revolution 20 ± 1r/min, rotation 1500 ± 50r/min, high-speed stirred revolution 25 ± 1r/min, rotation 2200 ± 50r/min, high-speed stirred vacuumizes and connects cool circulation water, suction-0.08 ~-0.09MPa, vacuum breaker degree 0 ~-0.01 MPa, slurry temperature controls below 50 DEG C.Slurry solid content 35%.For the first time, second time adds mixed raw material stirring at low speed 5min, high-speed stirred 1h, third time adds mixed raw material stirring at low speed 5min, high-speed stirred 2h, finally add NMP adjusting viscosity, viscosity is 5500MPas, stirring at low speed vacuum froth breaking, 200 mesh sieves crossed by slurry, obtain finely dispersed anode sizing agent.
Embodiment 2
By 2.5kg binding agent PVDF(France Arkema PVDF HSV900), 1.0kg conductive agent carbon nano-tube (Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences carbon nano-tube TNCC), 1.5kg Ketjen black (Japanese LION company ECP), 45kg rate lithium-iron phosphate active material (Heter Electronics Group Co., Ltd.'s self-control) V-type batch mixer VH-100(Nanjing Ke Dixin plant equipment Co., Ltd) mixing, rotating speed 10 ± 1r/min, mixing time 4h.Then mixed raw material is put into air blast baking box 85 ± 5 DEG C baking 10h, close heating make mixed raw material naturally cool to less than 45 DEG C for subsequent use, 116.7kgNMP is joined in 200L double-planet power mixer (Guangzhou good luck mixing apparatus Co., Ltd) agitator, then mixed raw material is divided to join for three times in double-planet power mixer agitator and stir, add the mixed raw material of about 1/3 at every turn, scrape wall after adding mixed raw material after first stirring at low speed 5min restart high-speed stirred and vacuumize at every turn, stirring at low speed revolution 20 ± 1r/min, rotation 1500 ± 50r/min, high-speed stirred revolution 25 ± 1r/min, rotation 2200 ± 50r/min, high-speed stirred vacuumizes and connects cool circulation water, suction-0.08 ~-0.09MPa, vacuum breaker degree 0 ~-0.01 MPa, slurry temperature controls below 50 DEG C.Slurry solid content 30.0%.For the first time, second time adds mixed raw material stirring at low speed 5min, high-speed stirred 1h, third time adds mixed raw material stirring at low speed 5min, high-speed stirred 2h, finally add NMP adjusting viscosity, viscosity is 4770MPas, stirring at low speed vacuum froth breaking, 200 mesh sieves crossed by slurry, obtain finely dispersed anode sizing agent.
Embodiment 3
By 3.0kg binding agent PVDF(France Arkema PVDF761A), 1.0kg conductive agent carbon nano-tube (Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences carbon nano-tube TNCC), 1.5kg superconduction carbon black Ensaco 350G(Switzerland Te Migao), 44.5kg rate lithium-iron phosphate active material (Heter Electronics Group Co., Ltd.'s self-control) V-type batch mixer VH-100(Nanjing Ke Dixin plant equipment Co., Ltd) mixing, rotating speed 10 ± 1r/min, mixing time 3h.Then mixed raw material is put into air blast baking box 85 ± 5 DEG C baking 10h, close heating make mixed raw material naturally cool to less than 45 DEG C for subsequent use, 88.9kgNMP is joined in 200L double-planet power mixer (Guangzhou good luck mixing apparatus Co., Ltd) agitator, then mixed raw material is divided to join for three times in double-planet power mixer agitator and stir, add the mixed raw material of about 1/3 at every turn, scrape wall after adding mixed raw material after first stirring at low speed 5min restart high-speed stirred and vacuumize at every turn, stirring at low speed revolution 20 ± 1r/min, rotation 1500 ± 50r/min, high-speed stirred revolution 25 ± 1r/min, rotation 2200 ± 50r/min, high-speed stirred vacuumizes and connects cool circulation water, suction-0.08 ~-0.09MPa, vacuum breaker degree 0 ~-0.01 MPa, slurry temperature controls below 50 DEG C.Slurry solid content 30.0%.For the first time, second time adds mixed raw material stirring at low speed 5min, high-speed stirred 1h, third time adds mixed raw material stirring at low speed 5min, high-speed stirred 2h, finally add NMP adjusting viscosity, viscosity is 5660MPas, stirring at low speed vacuum froth breaking, 200 mesh sieves crossed by slurry, obtain finely dispersed anode sizing agent.
Claims (1)
1. an anode slurry of high-rate preparation method, the steps include: binding agent PVDF, conductive agent, lithium-iron phosphate active material 1:(0.8 ~ 1.2 in mass ratio): (18 ~ 23) mix with V-type batch mixer, rotating speed 20 ± 1r/min, mixing time 2 ~ 4h, then mixed raw material is put into air blast baking box 85 ± 5 DEG C baking 8 ~ 12h, close heating make mixed raw material naturally cool to less than 45 DEG C for subsequent use, mixed raw material is divided in the agitator joining dress NMP for three times and stir with planetary mixer, first stirring at low speed after at every turn adding mixed raw material, start high-speed stirred after scraping wall and vacuumize, stirring at low speed revolution 20 ± 1r/min, rotation 1500 ± 50r/min, high-speed stirred revolution 25 ± 1r/min, rotation 2200 ± 50r/min, high-speed stirred vacuumizes and connects cool circulation water, suction-0.08 ~-0.09MPa, vacuum breaker degree 0 ~-0.01 MPa, slurry temperature controls slurry solid content below 50 DEG C and controls 30 ~ 40%, add mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 1 ~ 1.5h for the first time, for the second time, third time adds mixed raw material stirring at low speed 5 ~ 10min, high-speed stirred 2 ~ 3h, and finally add NMP adjusting viscosity, viscosity controls at 3000 ~ 6000mPas, stirring at low speed vacuum froth breaking, 200 mesh sieves crossed by slurry, obtain finely dispersed anode sizing agent.
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| CN103346311B (en) * | 2013-06-09 | 2015-04-29 | 浙江努奥罗新能源科技有限公司 | Manufacturing method for cathode material of lithium battery |
| CN104766948A (en) * | 2014-01-08 | 2015-07-08 | 中山天贸电池有限公司 | Processing method of lithium ion battery positive electrode slurry |
| CN103811764B (en) * | 2014-02-21 | 2016-01-13 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of anode sizing agent |
| CN105161676A (en) * | 2015-08-25 | 2015-12-16 | 田东 | Preparation method for lithium iron phosphate cathode slurry |
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| CN109962240A (en) * | 2017-12-25 | 2019-07-02 | 中国电子科技集团公司第十八研究所 | Method for preparing anode slurry for lithium carbon fluoride battery with carbon nanotube as conductive agent |
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| CN109817896A (en) * | 2019-04-08 | 2019-05-28 | 珠海冠宇电池有限公司 | A kind of preparation method and lithium ion battery of LiFePO4 anode of secondary cell |
| CN111081970B (en) * | 2019-12-25 | 2021-02-05 | 江西安驰新能源科技有限公司 | Slurry mixing process for improving solid content of slurry |
| CN111883736A (en) * | 2020-06-08 | 2020-11-03 | 惠州锂威新能源科技有限公司 | Preparation method of lithium ion battery anode slurry |
| CN112467128B (en) * | 2020-12-09 | 2022-07-26 | 山东精工电子科技有限公司 | Lithium titanate slurry for lithium battery and preparation method of lithium titanate slurry |
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